Phosgene → 2(2-n-Butoxyethoxy)-ethyl chloroformate

HRID 328330

반응식

HRID 328330 반응식
[CH2:1]([O:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][OH:11])[CH2:2][CH2:3][CH3:4].[C:12](Cl)([Cl:14])=[O:13]>C1C=CC=CC=1>[Cl:14][C:12]([O:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][O:5][CH2:1][CH2:2][CH2:3][CH3:4])=[O:13]

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 8177Diethylene Glycol Monobutyl Ether

생성물 1

HCID 138287912(2-n-Butoxyethoxy)-ethyl chloroformate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

24.3 G. (150 mmoles) of 2-(2-n-butoxyethoxy)ethanol is added dropwise with stirring to 250 ml. (290 mmoles) of a 12.5% phosgene solution in benzene, cooled in an ice bath and protected from moisture. The addition is carried out over a period of approximately 1 1/2 hours and stirring is continued in an ice bath for 2 hours. The solution is allowed to warm to room temperature and stirred overnight. Nitrogen is passed through the solution for several hours to remove excess phosgene and excess HCl. The solvent is removed in vacuo affording 32.9 g. of a colorless oil. The infrared spectrum revealed a strong carbonyl absorption and no hydroxy absorption. The oil is used without any further purification in the next step.

후처리

  1. additionThe addition
  2. stirringstirring
  3. waitis continued in an ice bath for 2 hours
  4. stirringstirred overnight
  5. waitNitrogen is passed through the solution for several hours
  6. customto remove excess phosgene and excess HCl
  7. customThe solvent is removed in vacuo
  8. customaffording 32.9 g
  9. customa strong carbonyl absorption
  10. customno hydroxy absorption
  11. customThe oil is used without any further purification in the next step

출처 및 근거

ORD 기록
ord-73c9eba9fb10439d8754a85b3b7f4ff9
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017503

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